Crystal growth and structural and optical characterizations of mixed-cation MA1−xCsxPbBr3 halide perovskite solid solutions
Abstract
Photovoltaic devices fabricated using mixed-cation halide perovskites have demonstrated a superior combination of high efficiency and long operating life. In this study, we synthesize a series of mixed-cation halide perovskites with the composition of MA1−xCsxPbBr3 (MA = CH3NH3), where x varies from 0 to 1. We carefully examine various polar solvents and develop a relatively facile, room temperature solution-based growth method for growing these single crystals under optimal conditions. We conduct a comprehensive investigation of the influence of the Cs+ cation on the structure and optical properties of the perovskite solid solutions. The structural characterization using X-ray diffraction confirms the successful substitution of cesium for the methylammonium (MA) cation in the MA1−xCsxPbBr3 perovskite structure, with a continuous solubility. As the Cs+ content increases, the crystal structure undergoes a gradual transformation from a cubic phase (for MAPbBr3) to an orthorhombic phase (for CsPbBr3). To study the impact of Cs substitution on their optical properties, we perform UV–Vis absorption analysis, and find no significant change in the bandgap value, which remains approximately 2.12–2.14 eV for the compositions with x up to 0.7. For x > 0.7, however, the bandgap value gradually increases to reach 2.21 eV for pure CsPbBr3. This work demonstrates a valid technique for the growth of halide perovskite solid solution crystals, which can be a versatile tool for tailoring the structure, long-term stability, and optoelectronic properties for advanced photovoltaic applications.
1. Introduction
Halide perovskite materials have revolutionized the fields of photovoltaics and optoelectronics due to their exceptional properties, such as high optical absorption, tunable bandgap, high carrier mobility, long carrier diffusion length, and excellent defect tolerance.1–4 Over the past decade, significant strides have been made in improving the power conversion efficiencies (PCE) of solar cells based on halide perovskites. These efficiencies have soared from a modest 3.8% for liquid dye-sensitized solar cells in 2009 5 to an exciting recent record of approximately 25% for solid-state perovskite solar cells.6 This remarkable progress, along with the low-cost feature of these materials, positions halide perovskites as promising candidates not only for solar cells 7 but also for various optoelectronic devices, including photodetectors,8 high-energy radiation detectors,9 light-emitting diodes,10 lasing devices,11 and photocatalysts.12
The general chemical formula of halide perovskite crystal structure is ABX3, where A and B represent cations, and X denotes Cl, Br, or I. Based on the nature of the A-site cation, halide perovskites can be categorized into organic–inorganic halide perovskites (OIHPs) and all-inorganic halide perovskites. Among them, OIHPs like CH3NH3PbX3 (X = I, Br, Cl) have received substantial attention, and the PCE of CH3NH3PbI3-based solar cells has exceeded 21%.7,13,14 Despite these impressive achievements, the organic methylammonium (MA) cation suffers from some inherent drawbacks, especially its sensitivity to moisture and oxygen, leading to the degradation of perovskite solar cells over time, which remains a critical challenge.15–17 To address the instability issue, several strategies, such as composition engineering,18–20 configuration engineering,21–23 single crystal growth,24–26 and device encapsulation, have been proposed and explored in recent years.
On the other hand, rapid progress has been made in research on mixed-cation and/or mixed-anion halide perovskites to achieve higher PCE and improved stability.27–29 The use of mixed halide perovskite solid solution materials offers several advantages, including enhanced device performance, prolonged operation lifetime, improved charge carrier properties, and tunable bandgap.30–34 Introducing cesium (Cs+) cations into OIHPs has been shown to enhance stability while maintaining a high PCE, for example 21% for Cs0.05 (MA0.17FA0.83)0.95 Pb(I0.83Br0.17)3, 20% for FA0.75Cs0.25Sn0.5Pb0.5I3, 19.23% for Cs0.10FA0.90PbI3, and 19% for FA0.75Cs0.25Sn0.5Pb0.5I3.18,35–37 Particularly intriguing is the achievement of the brightest and most efficient green light-emitting diode using the mixed-cation Cs0.87MA0.13PbBr3 perovskite.38
In the current landscape, most photovoltaic devices are based on polycrystalline perovskite films, composed of numerous crystalline grains with different orientations and grain boundaries. Unfortunately, those grain boundaries can facilitate ion migration, leading to poor device stability. In contrast, single crystals of halide perovskites have emerged as a superior alternative due to their enhanced carrier properties, such as high carrier mobility and long carrier diffusion length, as well as lower trap density.39–41 The absence of grain boundaries and the reduced defect density in single crystals further minimize ion migration, resulting in improved thermal stability and resistance to humidity.24 Consequently, synthesizing single crystals of mixed-cation halide perovskites becomes a compelling avenue for advancing photovoltaic performance.
Various methods have been developed for growing perovskite single crystals, including the inverse temperature crystallization (ITC),42 the anti-solvent vapor-assisted crystallization (AVC),41 and the Bridgman growth method.43 ITC is widely used for growing halide perovskite crystals at elevated temperatures (∼100 °C) due to the inverse solubility of these materials in specific polar solvents. While this method allows quick growth of small- to medium-sized crystals, obtaining large crystals often necessitates time-consuming seed-assisted growth, requiring multiple precursor solution replacements.44 Alternatively, the AVC method was used to grow mixed-cation MA1−xCsxPbBr3 single crystals that have demonstrated improved thermostability and enhanced device performance.45,46 Recently, we successfully developed a room temperature crystallization process, enabling the growth of MAPbBr3 and MAPbCl3 crystals in the DMF and DMSO solvents at room temperature, respectively.47 Additionally, we also grew the CsPbBr3 crystals in a mixed solvent of DMSO:DMF at room temperature.48
In this work, we present a novel solvent engineering strategy to grow mixed-cation MA1−xCsxPbBr3 (0 ≤ x ≤ 1) single crystals at room temperature. Through controlled solvent evaporation, we achieve optimal growth conditions by carefully considering the solubility behaviour of the compounds in various polar solvents, including DMSO, DMF, and their mixtures. Our approach overcomes the challenge of controlling the crystal composition associated with the conventional solution growth process for CsPbBr3, which usually requires a non-stoichiometric solution with excess PbBr2 to prevent the formation of non-perovskite phases.49,50 By employing a stoichiometric precursor ratio and engineered solvent, we successfully grow the MA1−xCsxPbBr3 single crystals at room temperature with precise control of the compositions. The crystal structure and phase purity are analyzed using high-resolution powder X-ray diffraction. UV–Vis spectroscopy is performed to investigate the effect of Cs+ substitution on their absorption edge and bandgap of the grown crystals.
2. Materials and methods
All the chemical reagents were purchased from Sigma–Aldrich and used as received without further treatment.
2.1. Growth of MA1−xCsxPbBr3 single crystals at room temperature
Firstly, a homogeneous precursor solution was meticulously prepared by dissolving equimolar amounts of ((1−x) MABr: xCsBr) and PbBr2 at maximum concentration in the DMSO–DMF-based solvents based on the compositions (see Table 1). The experimental determination of the optimum solvent and its maximum solubility was performed for each composition. The details of compositions, solvents, and solubility limits are provided in Table 1. Subsequently, the precursor solution was stirred at room temperature for a duration of 2 h. Next, the solution was transferred into a half-closed flask that was partially capped and allowed to sit at room temperature for 1 day to facilitate crystal growth. Remarkably, multiple crystals were successfully grown for each composition, as shown in Fig. 1.
Fig. 1.
Table 1.
2.2. High-resolution powder X-ray diffraction (PXRD) and UV–Vis absorption measurements
The initial step in powder X-ray diffraction (PXRD) involved crushing some grown crystals into fine powders. Subsequently, PXRD patterns were acquired using a Bruker D8 Advance Diffractometer, which was equipped with a Goebel mirror to generate a parallel X-ray beam for high-resolution diffraction analysis. For a comprehensive analysis of the crystal structure and lattice parameters, Pawley refinement was conducted using the TOPAS software package, focusing on both MAPbBr3 and CsPbBr3. To investigate the optical properties of the crystals, UV–Vis absorption measurements were performed at room temperature, using an FS5 spectrofluorometer, equipped with an SC-30 integrating sphere sample module, which facilitated accurate and reliable measurements of the UV–Vis absorption characteristics.
3. Results and discussion
3.1. Synthesis of MA1−xCsxPbBr3 single crystals
For the synthesis of the MA1−xCsxPbBr3 single crystals, a precursor solution comprising equimolar amounts of (1−x) MABr: xCsBr and PbBr2 was dissolved in a mixed solvent consisting of DMSO and DMF. Here, x represents the fraction of MABr being replaced by CsBr. To optimize the synthesis process, we initially screened several solvents to identify the optimum solvent composition that could dissolve all the precursors with their maximum solubility. The solvents tested included DMSO and DMF individually, as well as their mixtures with different ratios.
It is noteworthy that MAPbBr3 exhibits an absolute inverse solubility in DMF, limiting its maximum solubility to 1.5 M at room temperature, which is consistent with previous reports.42,44 Conversely, CsPbBr3 shows a good solubility in DMSO but a limited solubility in DMF. Our experimental tests revealed the maximum solubility values of 0.45 and 0.04 M for CsPbBr3 in DMSO and DMF, respectively, at room temperature. Attempts to grow pure CsPbBr3 crystals without by-products (i.e., 100% yield) have been challenging.49,50 When preparing the CsPbBr3 precursor solution in pure DMSO, only a few CsPbBr3 crystals formed, accompanied by a significant amount of undesired needle-shaped crystals. To improve the process, we investigated various mixed solvent ratios of DMSO:DMF for the CsPbBr3 crystal growth. The best result was achieved using a mixed solvent composition of 62 vol.% DMSO:38 vol.% DMF, yielding pure CsPbBr3 crystals without any trace of impurities. After conducting an extensive series of experiments, we have reached a conclusive finding that the MA1−xCsxPbBr3 perovskites exhibit a higher solubility when dissolved in mixed DMSO–DMF solvents. Table 1 presents the optimal solvent compositions for achieving the maximum solubility of various mixed-cation perovskite compositions at room temperature. The data offers valuable insights into the critical solvent mixtures required for successful crystal growth of these materials. As depicted in Table 1, an increase in the Cs+ content results in a reduction in the maximum solubility of the mixed halide perovskite. This decrease can be attributed to the limited solubility of CsBr in DMF, which acts as a limiting factor during the dissolution process.
Once the saturated precursor solution was prepared, it was transferred to a semi-sealed flask and kept at room temperature. Crystallization was driven by the supersaturation of the solution, achieved through slow solvent evaporation at room temperature. Nucleation occurred within a few hours, and the crystal growth process was completed within a few days. Figure 1 illustrates the schematic of the room-temperature growth method employed to obtain the crystals, along with the resultant crystals.
3.2. Structural evolution of the MA1−xCsxPbBr3 crystals
PXRD analysis was conducted at room temperature for the crystal series, with x ranging from 0 to 1. Figure 2a illustrates the PXRD patterns of various compositions, showing the effect of Cs substitution for MA on the crystal structure. All the compositions exhibit a perovskite structure without any secondary phases. The pure MAPbBr3 shows prominent diffraction peaks at 2θ values of ∼14.97°, 21.18°, 30.15°, and 33.82°, corresponding to the (100), (110), (200), and (210) crystal planes, respectively. By Pawley refinements, we confirm a perovskite structure of cubic symmetry, with the space group Pm
m and lattice parameter a = 5.922 Å, consistent with previous research works.42,51 Similarly, CsPbBr3 exhibits distinct split diffraction peaks at ∼(15.07°, 15.23°), (21.48°, 21.64°), (30.42°, 30.67°), and (34.15°, 34.36°), fully in agreement with the orthorhombic structure (Pnma, a = 8.234 Å, b = 11.722 Å, c = 8.179 Å) at room temperature, as reported previously.49,50 As the mole fraction of Cs increases from x = 0 (cubic MAPbBr3), the solid solution (100) diffraction peak shifts to higher 2θ values in the PXRD patterns with increasing Cs fraction up to x = 0.5. This shift is attributed to the smaller ionic radius of the Cs+ cation (0.188 nm) compared to the MA+ cation (0.217 nm), causing a reduction in the unit cell size and lattice parameters, leading to the peak shift to the right (i.e., to higher 2θ angles). With larger Cs fractions, the (100), (110), (200), and (210) diffraction peaks gradually transform from single peaks to double peaks, indicating an evolution of symmetry from the cubic phase of the MAPbBr3 origin to the orthorhombic of the CsPbBr3 origin. Figure 2b exemplifies the splitting of the (100) and (200) peaks into (020)/(101) and (040)/(202) peaks, respectively. The transformation occurs due to an octahedral rotation that takes place when the Cs content exceeds 50%, leading to an adjustment in its position and reducing the cubic to orthorhombic symmetry.
m and lattice parameter a = 5.922 Å, consistent with previous research works.42,51 Similarly, CsPbBr3 exhibits distinct split diffraction peaks at ∼(15.07°, 15.23°), (21.48°, 21.64°), (30.42°, 30.67°), and (34.15°, 34.36°), fully in agreement with the orthorhombic structure (Pnma, a = 8.234 Å, b = 11.722 Å, c = 8.179 Å) at room temperature, as reported previously.49,50 As the mole fraction of Cs increases from x = 0 (cubic MAPbBr3), the solid solution (100) diffraction peak shifts to higher 2θ values in the PXRD patterns with increasing Cs fraction up to x = 0.5. This shift is attributed to the smaller ionic radius of the Cs+ cation (0.188 nm) compared to the MA+ cation (0.217 nm), causing a reduction in the unit cell size and lattice parameters, leading to the peak shift to the right (i.e., to higher 2θ angles). With larger Cs fractions, the (100), (110), (200), and (210) diffraction peaks gradually transform from single peaks to double peaks, indicating an evolution of symmetry from the cubic phase of the MAPbBr3 origin to the orthorhombic of the CsPbBr3 origin. Figure 2b exemplifies the splitting of the (100) and (200) peaks into (020)/(101) and (040)/(202) peaks, respectively. The transformation occurs due to an octahedral rotation that takes place when the Cs content exceeds 50%, leading to an adjustment in its position and reducing the cubic to orthorhombic symmetry.Fig. 2.
Our PXRD analysis of the (100) diffraction peak reveals a notable trend in the lattice parameter “a” for the range of x between 0 and 0.5. Specifically, as the Cs content in the solid solutions increases, we observe a corresponding decrease in the lattice parameter “a”. This observation is consistent with the findings of Fan et al., who reported a similar behaviour in the growth of MA(1−x)CsxPbBr3 crystals.46 The systematic shift in the lattice parameter of the MA(1−x)CsxPbBr3 solid solutions over this limited composition range is also consistent with Vegard’s law, which states that the lattice parameter of a solid solution of two constituents is approximately a weighted mean of the two constituents’ lattice parameters. However, Vegard’s law strictly applies to constituents possessing the same crystal structure, so deviations from this behaviour would not be surprising given the MAPbBr3 (cubic symmetry) and CsPbBr3 (orthorhombic symmetry) end member structures. Indeed, for x > 0.50 the PXRD data indicate an orthorhombic structure, but with no significant structural changes with increasing Cs content. It should also be emphasized that growth of these crystals is subject to the added complexity of differential solubilities of MABr and CsBr from mixed solvents, suggesting the potential for a lack of proportionality between the concentration of MA cation dissolved in the initial solution and the amount incorporated in the mixed single crystals.
3.3. Optical properties of the MA1−xCsxPbBr3 crystals
To investigate the effect of Cs substitution for MA on the optical properties of the solid solution, UV–Vis absorption spectroscopy was performed on the MA1−xCsxPbBr3 crystals. As shown in Fig. 3, pure MAPbBr3 exhibits a sharp absorbance edge at 560 nm, while CsPbBr3 shows one at 540 nm. By fitting the data using the Tauc plot, we determine the optical bandgap (Eg) to be 2.12 eV for MAPbBr3 and 2.21 eV for CsPbBr3. Notably, these bandgap values are nearly equal to or slightly lower than those reported for single crystals prepared by other methods.42,49,52 The substitution of Cs results in a blue-shift of the absorption onset for the solid solutions, which can be attributed to the larger bandgap of the CsPbBr3 end member. Interestingly, for some mixed perovskites, the steepness of the absorption edge decreases, leading to an expansion of the absorbance edge over wider wavelength ranges.
Fig. 3.
Figure 3c shows the calculated bandgap values for the crystals. The optical bandgap of the MA1−xCsxPbBr3 perovskites increases gradually with increasing Cs content from 2.12 eV for MAPbBr3 to 2.21 eV for CsPbBr3, indicating that the bandgap can be tuned by controlling the concentration of Cs. Notably, we observe that the perovskite solid solutions with x values of 0.05, 0.1, 0.4, 0.6, and 0.7 exhibit similar bandgap values of 2.13–2.14 eV, closely resembling that of the pure MAPbBr3. This phenomenon can be attributed to their broad absorption edges, which may influence the slope values extracted from the Tauc plot. The bandgap value increases with x ≥ 0.8, reaching that of CsPbBr3.
We have conducted an analysis of the Urbach energy (EU) for each composition studied. The Urbach energy serves as an important metric offering insights into the degree of energetic disorder within the material and can provide information on the potential presence of tail states near the band edge. By determining the Urbach energy from the UV–Vis spectra, we aim to understand the variations in the sharpness or breadth of transitions at the band edges for different compositions. The extraction of Urbach energy values involves fitting the exponentially decaying tail of the absorption spectrum near the band edge, as illustrated in Fig. 3d. Our analysis reveals a notable range of Urbach energies, spanning from 24 to 125 meV (see Fig. 3c).
The variations in the Urbach energy correlate with the observed differences in the slope of the UV–Vis spectra, reflecting the degree of energetic disorder and the potential presence of tail states near the band edges. The end member MAPbBr3 and CsPbBr3 single crystals display the sharpest absorption onsets and correlate well with the lowest observed Urbach energies anticipated from materials with compositional uniformity and relatively low degrees of energetic disorder. With increasing Cs fraction in the range 0 < x < 0.5, the Urbach energy is relatively constant at approximately 70 meV but elevated significantly from those of the end members. With increasing Cs composition beyond this range, the Urbach energy is observed to increase dramatically to a maximum of approximately 125 meV at x = 0.7, before decreasing again as x approaches 1.0. Interestingly, the observed Urbach energies of the solid solutions are uniformly greater than the compositionally pure end members but appear to be significantly larger for solid solutions with x > 0.5 compared to those with x < 0.5. This correlates with the structural parameters of the solid solutions in that compositions with x > 0.5 are orthorhombic in structure while solid solutions of smaller Cs fraction are cubic. To the extent that the energetic disorder is a reflection of structural disorder in these systems, the observation of greater Urbach energies for the orthorhombic solid solutions may reflect the higher degree of structural disorder that accompanies a structure of lower symmetry. However, this structural disorder does not include that due to localized states, defects, or other structural imperfections that may result during the crystallization process.
Nevertheless, our findings underscore the importance of considering energetic disorder in the interpretation of the UV–Vis results. In light of the Urbach energy analysis, we acknowledge the potential influence of disorder on the reliability of extrapolated bandgap values. Changes in Urbach energy can impact the accuracy of the bandgap values determined, particularly when tail states contribute significantly to the observed optical transitions, increasing the level of uncertainty on band gap determinations that rely solely on optical measurements. These observations highlight the interplay between the energetic disorder and the optical properties in the MA(1−x)CsxPbBr3 perovskite solid solutions.
4. Conclusions
In this study, we have successfully synthesized the single crystals of mixed-cation perovskite solid solutions of MA1−xCsxPbBr3 with varying compositions (x = 0, 0.05, 0.1, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, and 1), by a novel and efficient room-temperature growth technique through controlled solvent evaporation. The growth conditions were optimized through an in-depth investigation of solubility and supersaturation behaviour, leading to the identification of the optimum solvent compositions with the maximum solubility concentration for each composition. The crystal structure and phase purity of the MA1−xCsxPbBr3 perovskites were thoroughly examined using X-ray diffraction analysis at room temperature. Notably, all the compositions exhibit a typical perovskite structure, indicating successful substitution of the Cs cation for the MA cation into the perovskite lattice, forming a series of continued solid solutions. The (100) diffraction peak characteristic of pure cubic perovskite MAPbBr3 shifts systematically to higher diffraction angles for solid solutions with increasing Cs fraction, which is attributed to a shrinking of the unit cell due to the smaller size of the Cs cation compared with that the MA cation. For the compositions with x > 0.5, the appearance of split peaks indicates a transformation of the crystal structure from the cubic phase of the MAPbBr3 origin to the orthorhombic phase of the CsPbBr3 origin. Therefore, the substitution of Cs+ ion for MA+ induces a structural crossover from the cubic to orthorhombic phase in the MA1−xCsxPbBr3 solid solutions at the critical composition of x = 0.5. The optical properties of the MA1−xCsxPbBr3 crystals were investigated through UV–Vis absorption spectral measurements. The spectra reveal a blue-shift of approximately 20 nm from MAPbBr3 to CsPbBr3. While the pure MAPbBr3 and CsPbBr3 show a sharp absorbance edge in their optical spectra, it is observed that the mixed-cation perovskites display a gradual broading in the absorbance edge. Based on an Urbach energy analysis, we attribute the broad bandgap onsets to tail states appearing in the bandgap region that are associated with energy disorder in the solid solutions. The magnitudes of these Urbach energies suggest that the degree of disorder in the perovskite systems is significantly greater for the orthorhombic solid solutions associated with Cs fractions > 0.5 than for solid solutions with cubic structure observed at lower Cs compositions. This phenomenon has significant implications on their optical bandgap properties and increases significantly the uncertainty in their accurate determination. Nevertheless, the bandgap analysis based on the Tauc plot indicates that crystals with compositions of MA1−xCsxPbBr3 (x = 0, 0.05, 0.1, 0.4, 0.6, and 0.7) have similar bandgap values to that of pure MAPbBr3 (∼2.12–2.4 eV). Our findings suggest that these crystals could effectively maintain a good light harvesting efficiency while benefiting from an improved chemical stability thanks to the partial substitution of Cs for MA.
Acknowledgements
This work was supported by the Natural Sciences and Engineering Research Council of Canada (NSERC; Discovery Grant Nos. RGPIN-2023-04416, RGPIN-2023-05827, and RGPIN-2018-05800) and the U. S. Office of Naval Research (ONR; Grant No. N00014-21-1-2085).
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Information & Authors
Information
Published In
Canadian Journal of Chemistry
Volume 102 • Number 6 • June 2024
Pages: 366 - 373
History
Received: 28 October 2023
Accepted: 29 January 2024
Accepted manuscript online: 16 March 2024
Version of record online: 1 May 2024
Copyright
© 2024 The Author(s). This work is licensed under a Creative Commons Attribution 4.0 International License (CC BY 4.0), which permits unrestricted use, distribution, and reproduction in any medium, provided the original author(s) and source are credited.
Data Availability Statement
Data generated or analyzed during this study are provided in full within the published article.
Key Words
Authors
Author Contributions
Formal analysis: MB, YL
Funding acquisition: ZGY, GWL, DBL
Methodology: JJER, MB, JAP
Supervision: DBL, GWL, ZGY
Validation: GWL
Writing – original draft: MB
Writing – review & editing: GWL, ZGY
Competing Interests
The authors declare there are no competing interests.
Funding Information
Natural Sciences and Engineering Research Council of Canada: RGPIN-2018-05800, RGPIN-2023-04416, RGPIN-2023-05827
Office of Naval Research: N00014-21-1-2085
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Maryam Bari, Jessy J.E. Ruan, Yihan Lin, Jefferson A. Pells, Gary W. Leach, Daniel B. Leznoff, and Zuo-Guang Ye. 2024. Crystal growth and structural and optical characterizations of mixed-cation MA1−xCsxPbBr3 halide perovskite solid solutions. Canadian Journal of Chemistry.
102(6): 366-373. https://doi.org/10.1139/cjc-2023-0193
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